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Preparation method for extracting and separating emetini hydrochloridium and cephaeline hydrochloride from ipecace

A technology for emetine hydrochloride and emetine hydrochloride, which is applied in the field of extracting and refining emetine hydrochloride and emetine hydrochloride, and can solve problems not involved in the extraction and refining methods of emetine hydrochloride and emetine hydrochloride , to achieve the effect of stable and controllable purification process, high stability and easy operation

Active Publication Date: 2012-08-15
JING JING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has been reported that ultrasonic extraction of ipecac with ethanol can effectively extract ether-soluble total alkaloids [Xu Liying, Song Weifeng, Research on Extraction Technology of Ether-soluble Alkaloids, Preparations and Technology, Volume 8, Issue 11, April 2011] But Ether-soluble alkaloids include many components, and do not involve the extraction and refining methods of emetine hydrochloride and emetine hydrochloride

Method used

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  • Preparation method for extracting and separating emetini hydrochloridium and cephaeline hydrochloride from ipecace
  • Preparation method for extracting and separating emetini hydrochloridium and cephaeline hydrochloride from ipecace
  • Preparation method for extracting and separating emetini hydrochloridium and cephaeline hydrochloride from ipecace

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Experimental program
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Effect test

Embodiment 1

[0058] 1. Extraction and separation

[0059] 1. Instruments and materials: ultrasonic extractor: preparative HPLC: LC-8A preparative chromatograph, SPD-M10A detector (Shimadzu, Japan); rotary evaporator RE-3000 (Shanghai Yarong Biochemical Instrument Factory); lyophilizer ALPHA 1-4LD (Christ, Germany).

[0060] Medicinal materials: ipecac, produced in Costa Rica, crushed and passed through a No. 3 sieve.

[0061] 2. Extraction of total alkaloids

[0062] A. Take 10 g of the pulverized medicinal material, add 200 ml of 70% acidic ethanol (2 ml of HCL is added to 70% ethanol), and perform ultrasonic extraction for 1 hour;

[0063] B. Centrifuge the extract, take the supernatant, evaporate the ethanol under reduced pressure at 40°C with a rotary evaporator, concentrate to 50ml, and adjust the pH value to 10 by adding ammonia test solution;

[0064] C. Extract with diethyl ether 4 times, 50ml each time, collect the diethyl ether layer, evaporate the solvent in a water bath, and...

Embodiment 2

[0073] 1. Extraction and separation

[0074] 1. Instruments and materials: ultrasonic extractor; liquid phase preparation: American Waters 2535 detector: 2489 ultraviolet detector; rotary evaporator RE-3000 (Shanghai Yarong Biochemical Instrument Factory); freeze dryer ALPHA 1-4LD (Germany christ ).

[0075] Medicinal materials: ipecac, produced in Costa Rica, crushed and passed through a No. 2 sieve.

[0076] 2. Extraction of total alkaloids

[0077] A. Take 10g of crushed medicinal materials, add 300ml of 3% acidic ethanol, the ethanol concentration is 90%, and ultrasonically extract for 2 hours;

[0078] B. Centrifuge the extract, take the supernatant, evaporate the ethanol under reduced pressure at 60°C with a rotary evaporator, concentrate to 30ml, and adjust the pH value to 12 by adding ammonia test solution;

[0079] C. Extract with ether 3 times, 30ml each time, collect the ether layer, evaporate the solvent in a water bath, and dilute the residue to a 10ml measurin...

Embodiment 3

[0086] 1. Extraction and separation

[0087] 1. Instruments and materials: ultrasonic extractor; preparative liquid phase: American varian 940 LC detector: Prostar 325 ultraviolet detector; rotary evaporator RE-3000 (Shanghai Yarong Biochemical Instrument Factory); freeze dryer ALPHA 1-4LD ( German Christ).

[0088] Medicinal materials: ipecac, produced in Costa Rica, crushed and passed through a No. 3 sieve.

[0089] 2. Extraction of total alkaloids

[0090] A. Take 10g of crushed medicinal materials, add 100ml 2% acidic ethanol, the ethanol concentration is 60%, and ultrasonically extract for 0.5 hours;

[0091] B. Centrifuge the extract, take the supernatant, evaporate the ethanol under reduced pressure at 50°C with a rotary evaporator, concentrate to 40ml, and adjust the pH value to 11 by adding ammonia test solution;

[0092] C. Extract with ether 3 times, 40ml each time, collect the ether layer, evaporate the solvent in a water bath, and dilute the residue to a 10ml m...

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Abstract

The invention discloses a preparation method for separating emetini hydrochloridium and cephaeline hydrochloride from ipecace. The maguireothamnus speciosus ipecace has the functions of being emetic, antitussive and expectorant, and contains six alkaloids such as emetini hydrochloridium, cephaeline hydrochloride and the like at present. The preparation method provided by the invention can be used for preparing the emetini hydrochloridium and cephaeline hydrochloride with the content which is more than 98% from the ipecace by the following steps of extracting, purifying, freeze drying, etc.

Description

technical field [0001] The invention relates to a method for extracting and refining emetine hydrochloride and emetine hydrochloride from ipecac. Background technique [0002] Ipeca is a perennial evergreen dwarf shrub belonging to Rubiaceae, belonging to the genus Caucus. The roots are twisted and cylindrical, dark brown, the stems are green, the branches are soft, and the flowers are white. The ipecac is mainly produced in the humid forests of Brazil, and the trade name is Brazilian ipecac. Ipeca root has been successfully planted in Bengal, Myanmar, the Federation of Malaya, Singapore, Indonesia and other places in eastern India, and it has also been introduced and cultivated in Guangdong, Yunnan, and Taiwan in my country. [0003] Ipeca root mainly contains ether-soluble total alkaloids, among which emetine hydrochloride and emetine hydrochloride are the main ones. Ipecaac is a medicine of the Indians in South America. It was introduced to Europe in 1672. It is consid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D455/00
Inventor 宋剑裴彩云王宗权韩桂茹贾永鑫
Owner JING JING PHARMA
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